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WO2015119954A1 - Substances et méthodes de remplacement d'un matériau de dent naturelle - Google Patents

Substances et méthodes de remplacement d'un matériau de dent naturelle Download PDF

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Publication number
WO2015119954A1
WO2015119954A1 PCT/US2015/014271 US2015014271W WO2015119954A1 WO 2015119954 A1 WO2015119954 A1 WO 2015119954A1 US 2015014271 W US2015014271 W US 2015014271W WO 2015119954 A1 WO2015119954 A1 WO 2015119954A1
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WIPO (PCT)
Prior art keywords
trioxide aggregate
mineral trioxide
mta
equal
anhydrous
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PCT/US2015/014271
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English (en)
Inventor
Mahmoud Torabinejad
Homayoun Moaddel
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Loma Linda University
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Loma Linda University
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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/50—Preparations specially adapted for dental root treatment
    • A61K6/56—Apical treatment
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/15—Compositions characterised by their physical properties
    • A61K6/17—Particle size
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/50—Preparations specially adapted for dental root treatment
    • A61K6/54—Filling; Sealing
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/849—Preparations for artificial teeth, for filling teeth or for capping teeth comprising inorganic cements
    • A61K6/851—Portland cements
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/849—Preparations for artificial teeth, for filling teeth or for capping teeth comprising inorganic cements
    • A61K6/853—Silicates

Definitions

  • This disclosure generally relates to dental materials and to dental materials for filling and sealing.
  • the enamel of a tooth is the intensely hard calcareous (i.e., calcium based) substance that forms a thin layer that caps or partly covers the teeth.
  • the enamel is the hardest substance of the animal body and its strength allows a tooth to perform its function over many years. The hardness of the enamel also serves to protect the sensitive living tissue within the tooth.
  • Dentin also comprises calcareous material similar to bone but harder.
  • Dentin is a living tissue comprised of a matrix of minute tubules which enter into the inner cavity of the tooth where the living tissues are housed.
  • the "pulp" of the tooth comprises the living or viable tissues of the tooth that are contained within the pulp cavity.
  • the pulp cavity comprises the pulp chamber, located near the crown of the tooth, and the root canal, which extends down to the very proximal or periapical regions of the tooth.
  • the pulp is comprised of connective tissue, blood vessels which nourish the tooth, and nerves that transmit pain and other signals to the brain. The blood vessels and nerves enter the tooth at the tip or apical section of the root canal. Depending upon the type of tooth, there is significant circulation of living matter within the pulp of the tooth.
  • the cementum is a thin, fairly hard bone tissue covering the root of the tooth. Surrounding the cementum is the periodontal ligament which serves to mount the tooth in the bony socket or alveolus, which is formed in the alveolar bone or jaw bone in which the teeth are set.
  • Dental decay is most likely to affect the enamel, dentin, and/or pulp. Once dental caries is found in the enamel, the typical therapy is to remove it in order to prevent the decay from penetrating the tooth. Such penetration could spread infection throughout the mouth and the body, and possibly result in loss of the tooth.
  • the therapy for cavities formed by decay is typically referred to as a "filling.”
  • a dentist or other experienced practitioner drills out the cavity formed by the decaying material.
  • a dentist may form undercuts in order to secure the subsequently applied filling material. The dentist then fills the cavity with a filling material which replaces the portion of the tooth lost to decay. The filling material is placed downward into the tooth from the upper or crown regions of the tooth, and is typically referred to as an "orthograde" filling. The dentist then packs the filling material densely and shapes it appropriately.
  • Root canal therapy is not always successful. It is estimated that in about 20-30% of cases, infection returns. This is usually caused by the migration of bacteria and other infectious organisms from the mouth along the root canal cavity. The bacteria migrates through the interstices of the canal to the living periapical tissues which remain following the root canal therapy. Furthermore, the root canal system is complex and cannot always be completely cleaned with present techniques and instruments. Thus, periapical abscesses may again form at the tip of the root canal. In these cases, the interstitial seal between the orthograde filling material and the walls of the root canal is not sufficient to prevent the invasion of infectious matter.
  • MTA mineral trioxide aggregate
  • an MTA mix can include a combination of MTA compounds with different particle sizes and uniformities.
  • the MTA mix sets in a relatively short time.
  • Some embodiments include a method for using an MTA mix in general dentistry and in endodontics.
  • the methods include using the MTA mix to fill a space in the tooth.
  • Some embodiments provide a method of making anhydrous high-shear homogenized mineral trioxide aggregate ("homogenized MTA").
  • the methods decrease particle size of the MTA.
  • the methods increase the uniformity of particle sizes of the MTA.
  • the methods include using a machine that homogenizes by high shear and impact impingement of particles.
  • Some embodiments provide a leak-resistant MTA mix.
  • the mix includes MTA and calcium sulfate.
  • the mix includes homogenized MTA and calcium sulfate.
  • an anhydrous fast set MTA mix comprises at least one of bismuth oxide, dicalcium silicate, tricalcium aluminate, and tricalcium silicate.
  • the fast set MTA mix is combined with an aqueous solution.
  • the anhydrous fast set MTA mix sets in less than or equal to about twenty minutes.
  • the fast set MTA mix sets in greater than or equal to about five minutes.
  • combining the anhydrous fast set MTA mix with an aqueous solution produces a dental substance for use in general dentistry and in endodontics to replace natural tooth material.
  • an anhydrous fast set MTA comprises an untreated MTA and a homogenized MTA.
  • a homogenized MTA has homogenized particles having a reduced median maximum particle diameter compared to untreated MTA.
  • the homogenized MTA is prepared by high-shear and impact impingement of particles. In some embodiments, the high- shear homogenization does not involve the use of grinding media.
  • untreated MTA comprises greater than or equal to about 15 wt. % and less than or equal to about 99 wt. % of the anhydrous fast set MTA mix.
  • homogenized MTA comprises greater than or equal to about 1 wt. % and less than or equal to about 85 wt. % of the anhydrous fast set MTA mix.
  • an anhydrous fast set MTA mix comprises greater than or equal to about 55 wt. % and less than or equal to about 85 wt. % untreated MTA and greater than or equal to about 15 wt. % and less than or equal to about 45 wt. % homogenized MTA.
  • a non-aqueous liquid is used in preparing a homogenized MTA or an anhydrous high-shear homogenized MTA mix.
  • the median maximum particle diameter of the untreated mineral trioxide aggregate is between about five and about thirty times larger than the median maximum particle diameter of the homogenized MTA.
  • the median maximum particle diameter of the untreated MTA is between about five and about fifteen times larger than the median maximum particle diameter of the homogenized MTA.
  • the anhydrous fast set MTA mix sets in about five to about twenty minutes when combined with an aqueous solution to produce a dental substance for use in general dentistry and in endodontics to replace natural tooth material.
  • the anhydrous fast set MTA mix includes tetracalcium alumino-ferrite.
  • a dental substance comprises anhydrous fast set MTA mix and an aqueous solution.
  • the anhydrous fast set MTA mix includes greater than or equal to about 50 wt. % of the dental substance.
  • the dental substance includes less than or equal to about 95 wt. % of the anhydrous fast set MTA mix in an aqueous solution.
  • the dental substance includes an aqueous component that is greater than or equal to about 5 wt. % of the aqueous solution.
  • the dental substance include an aqueous component that is less than or equal to about 50 wt. % of the aqueous solution.
  • a method for using the dental substance in general dentistry and in endodontics comprises performing a dental procedure, using a dental substance to fill a space in the tooth, and allowing the dental substance to set in between five to twenty minutes.
  • the dental procedure includes removing part of the natural tooth material of a tooth.
  • the dental procedure includes removing material that replaced natural tooth material.
  • a method for using the dental substance in general dentistry and in endodontics further comprises, after allowing the dental substance to set, adjusting the height of the dental substance in the tooth and carving the dental substance.
  • the dental procedure is an endodontic procedure.
  • the dental procedure includes at least one of the following: apexification, pulp capping, pulpotomy, regenerative endodontics, root canal filling, root-end filling, root perforation repair, and orthograde filling.
  • a method of making homogenized MTA comprises mixing untreated MTA with a non-aqueous liquid to produce a suspension of the untreated MTA and the non-aqueous liquid in a ratio of 1 part MTA to between 1 and 100 parts non-aqueous liquid, placing the suspension of the MTA into a machine that homogenizes by high-shear and impact impingement of particles, repeatedly forcing the suspension through the machine between two and 100 hundred times, and evaporating the non-aqueous liquid from the homogenized MTA to create homogenized MTA.
  • repeated contact of the particles with each other and with the machine reduces the size of the particles.
  • the homogenized MTA has a dlO value - which is defined as a maximum particle diameter that is greater than the maximum particle diameter of 10% of the particles - and a d90 value - which is defined as a maximum particle diameter that is greater than the maximum particle diameter of 90% of the particles.
  • methods of making homogenized MTA reduce the dlO value of the homogenized MTA to a value that is greater than or equal to about 0.05 ⁇ . In some embodiments, methods of making homogenized MTA reduces the dlO value of the aggregate to a value that is less than or equal to about 0.5 ⁇ .
  • the methods reduce the d90 value of the homogenized MTA to a value that is less than or equal to about 5 ⁇ .
  • methods of making homogenized MTA do not include ball milling. In some embodiments, the methods achieve a more uniform particle size distribution than a method that includes ball milling. In some embodiments, methods of making anhydrous homogenized MTA produces fewer particles with a maximum particle diameter larger than 5 ⁇ compared to particles reduced in size by ball milling. In some embodiments, methods of making homogenized MTA takes less time to reduce mean maximum particle diameter of an MTA to a desired mean maximum particle diameter than ball milling.
  • the methods of making homogenized MTA utilize a non-aqueous liquid comprising alcohol.
  • the MTA is mixed with a non-aqueous liquid in a ratio of about 1 part MTA to between about 1 and about 20 parts non-aqueous liquid.
  • methods include circulating the suspension through the machine between about two and about fifty cycles.
  • methods of making a fast set MTA mix for use in general dentistry and endodontics to replace natural tooth material comprises mixing a homogenized MTA with untreated MTA.
  • a leak-resistant MTA mix comprises at least one of bismuth oxide, dicalcium silicate, tricalcium aluminate, tricalcium silicate, and calcium sulfate.
  • combining the leak-resistant MTA mix with an aqueous solution produces a dental substance for use in general dentistry and in endodontics to replace natural tooth material.
  • the leak-resistant MTA mix comprises a homogenized MTA comprising homogenized particles having a reduced median maximum particle diameter compared to an untreated MTA.
  • a medical grade homogenized MTA is prepared by a process called high-shear homogenization, which involves high-shear and impact impingement of particles, which, in some embodiments, does not include the use of grinding media.
  • the median maximum particle diameter of the untreated MTA is between about five and about thirty times larger than the median maximum particle diameter of the homogenized MTA.
  • the MTA mix is leak-resistant and comprises calcium sulfate.
  • calcium sulfate is present in an amount greater than or equal to about 5 wt. % and less than or equal to about 15 wt. % of the leak-resistant MTA.
  • the leak-resistant MTA that includes calcium sulfate undergoes greater volumetric expansion during setting than an MTA without calcium sulfate.
  • the calcium sulfate in the leak-resistant MTA mix comprises at least one of calcium sulfate hemihydrate, calcium sulfate dihydrate, and calcium sulfate anhydrite. In some embodiments, the leak-resistant MTA mix comprises greater than or equal to about 5 wt. % calcium sulfate. In some embodiments, the leak-resistant MTA mix comprises less than or equal to about 10 wt. % calcium sulfate. In some embodiments, the leak-resistant MTA mix comprises about 10 wt. % calcium sulfate. In some embodiments, the leak-resistant MTA mix undergoes volumetric expansion of greater than about 0.5% during setting.
  • the substances may be used in general dentistry and in endodontics to replace natural tooth material.
  • the substances include a combination of MTA compounds each with a different fineness.
  • the substances include untreated MTA and homogenized MTA.
  • the homogenized MTA is anhydrous high-shear homogenized MTA, where the untreated MTA and anhydrous high- shear homogenized MTA together comprise an anhydrous fast set MTA mix.
  • the substance is a cement composition that can include at least one of bismuth oxide, dicalcium silicate, tricalcium aluminate, and tricalcium silicate.
  • the substance includes tertracalcium alumino-ferrite.
  • the cement composition includes calcium sulfate.
  • the cement composition includes Portland cement, or variations in the composition of such cement that exhibit favorable physical attributes sufficient to form an effective seal against reentrance of infectious organisms.
  • the cement composition does not include any additives, such as for example calcium phosphate.
  • the cement composition does not include a resin.
  • the substance includes an aqueous liquid.
  • the aqueous solution comprises water.
  • the water comprises distilled water.
  • the water includes at least one of deionized water, filtered water, slurry water, and tap water.
  • the aqueous solution comprises a local anesthetic, such as for example lidocaine hydrochloride, with or without epinephrine bitartrate.
  • lidocaine hydrochloride with or without epinephrine bitartrate.
  • other local anesthetics can be used in addition or in lieu of lidocaine hydrochloride, as will be understood by skilled artisans.
  • the setting time of the substance is controlled by adjusting the fineness of the dental substance.
  • the fineness of the dental substance is controlled by combining homogenized dental substance with untreated dental substance.
  • the fineness of the dental substance is controlled by homogenizing the dental substance.
  • the fineness of the dental substance is controlled by increasing or decreasing the number of homogenization cycles.
  • methods include using a dental substance comprising a fast set MTA mix to fill a space in the tooth, and allowing the substance to set.
  • methods include, before using the substance to fill a space in the tooth, applying an additive.
  • methods include, before using the substance to fill a space in the tooth, mixing the substance with an additive.
  • methods include mixing the substance with an additive before using the substance to fill a space in the tooth.
  • the additive is a radiopaque material, such as, for example, a phosphate. Other radiopaque materials can also be used, as will be understood by skilled artisans.
  • the additive does not compromise the biocompatibility of the fast set MTA mix.
  • the additive is an expanding agent, such as a sulfate.
  • the expanding agent is calcium sulfate.
  • the calcium sulfate is an anhydrite.
  • the calcium sulfate is a hemihydrate.
  • the calcium sulfate is a dihydrate.
  • the calcium sulfate is an anhydrite.
  • the expanding agent is gypsum. In some embodiments, adding the calcium sulfate to the fast set MTA mix does not compromise the biocompatibility of the MTA mix. In some embodiments, adding the calcium sulfate to the fast set MTA mix does not compromise the bioactivity of the MTA mix.
  • methods include orthograde filling.
  • method includes, after allowing the dental substance to set, adjusting the height of the dental substance in the tooth.
  • methods also include, after allowing the dental substance to set, carving the dental substance.
  • a method for making a substance for use in general dentistry and in endodontics to replace natural tooth material, where the substance sets in a relatively short time - minutes as compared to hours.
  • the particle size of the substance is reduced.
  • homogenization by high-shear and impact impingement of particles is used to reduce particle size, thereby producing anhydrous high-shear homogenized MTA.
  • methods for making a substance for use in general dentistry include mixing MTA with a non-aqueous liquid to produce a suspension of the MTA.
  • the non-aqueous liquid is an alcohol.
  • the method includes placing the suspension of the mineral trioxide aggregate into an inlet reservoir of a machine that homogenizes by high-shear and impact impingement of particles.
  • methods include operating a pump within the machine and accelerating the suspension into an interaction chamber using pressure.
  • methods also include forcing the suspension through a channel within the interaction chamber, wherein repeated contact of the particles with each other and with the channel walls reduces the size of the particles.
  • methods include circulating the suspension forced through the channel into the inlet reservoir between two and one hundred times. In some embodiments, methods include evaporating the non-aqueous liquid from the high-shear homogenized MTA to create anhydrous high-shear homogenized MTA.
  • a method for making a substance for use in general dentistry and in endodontics to replace natural tooth material, where the substance expands during setting.
  • methods include mixing mineral trioxide aggregate with calcium sulfate to produce a leak-resistant MTA mix.
  • methods include adding calcium sulfate to untreated MTA.
  • methods include homogenizing a mixture of calcium sulfate and untreated MTA.
  • methods include milling a mixture of calcium sulfate and untreated MTA by using a ball mill.
  • methods include adding calcium sulfate to an anhydrous fast set MTA mix having untreated MTA and homogenized MTA.
  • methods include adding homogenized MTA to the leak-resistant MTA mix. In some embodiments, methods include adding calcium sulfate to an aqueous solution to produce a calcium sulfate suspension. In some embodiments, methods include adding the calcium sulfate suspension to untreated MTA. In some embodiments, methods include adding the calcium sulfate suspension to high-pressure sheared MTA. In some embodiments, methods include adding the calcium sulfate suspension to an anhydrous fast set MTA mix.
  • FIG. 1 is a cross-section of a single-rooted tooth after apicoectomy and retrograde filling.
  • FIG. 2 is a schematic diagram of a combination of mineral trioxide aggregate compounds each with a different fineness or particle size.
  • FIG. 3 is a flow chart illustrating a method of reducing the particle size of a dental substance according to the present disclosure.
  • FIG. 4 is a schematic graph illustrating particle size distributions of untreated MTA compared with samples of homogenized MTA
  • FIG. 5 is a schematic graph illustrating a relationship between setting time and particle size.
  • FIG. 6 is a flow chart illustrating a method for using a dental substance according to the present disclosure.
  • a tooth filling material may exhibit any number of qualities. In some embodiments, it exhibits good adherence and adaptability to the tooth walls of the cavity. In some embodiments, it is compatible with the surrounding tissue and does not cause staining or other adverse effects to the surrounding tooth structure. In some embodiments, it hardens to provide structural support for the tooth, including its biting surface. In some embodiments, it is relatively easy to apply in an environment with blood, moisture, and potential access problems. In some embodiments, a filling material be radiopaque, i.e., exhibit a high absorption of the short wavelength x-ray radiation utilized in dental diagnostics. In some embodiments, it is sterile or easily sterilized.
  • the fluid and bacteria that are already present in the mouth may be kept away from reentering the cavity and causing further decay.
  • the chosen filling material adequately seals the cavity to prevent the migration of such fluid and bacteria into the cavity.
  • this sealing ability of the filling material can be used when the decay has caused access to the pulp of the tooth.
  • retrograde filling materials As with other types of fillings and root canals, various materials have been suggested as retrograde filling materials.
  • An ideal retrograde filling material may have many of the same qualities found in an orthograde filling material. It may adhere and adapt to the dentinal walls of the root end preparations, may prevent leakage of microorganisms and their byproducts into the periapical tissues, and may be biocompatible with the periapical tissues. It may also be insoluble in tissue fluids, dimensionally stable, and unsusceptible to the presence of moisture. Any antimicrobial qualities may be beneficial as they would inhibit infection and abscess.
  • retrofilling materials consist of many of the standard orthograde dental filling materials, and include gutta percha, zinc oxide eugenol paste, cavity, composite resins, gold foil, glass ionomers, standard amalgams, and other materials.
  • gutta percha zinc oxide eugenol paste
  • cavity composite resins
  • gold foil gold foil
  • glass ionomers standard amalgams
  • other materials The suitability of these materials as retrograde filling materials has been tested by their sealing ability, marginal adaption to the dentinal walls, biocompatibility, and their clinical performance. To date, many of these materials have been found wanting.
  • amalgam has been the most commonly used retrograde filling material for many years despite its many disadvantages.
  • One of its primary disadvantages is the allowance of initial leakage.
  • the amalgam When initially applied the amalgam has poor adaption to the dentinal cavity walls and allows leakage between the interface of the amalgam and dentinal walls. This leakage reduces over time due to secondary corrosion as the interface is exposed to the oral fluids. Even with secondary corrosion, the effectiveness of the seal has been questioned, and the corrosion products in the gap between the amalgam and the cavity walls may themselves be detrimental.
  • ZOE zinc oxide eugenol
  • Super EBA and IRM have also been used as retrograde filling materials.
  • the disadvantages of ZOE-based cements include moisture sensitivity, irritation of vital tissue, solubility, need for an undercut in the cavity preparation, and difficulty in clinical handling of the material.
  • Certain materials may be unsuitable to repair and reconstruct hard tissue of the anatomy.
  • Certain dental filling and sealing materials cannot be applied in an orthograde and/or retrograde cavity.
  • Certain materials do not satisfy the ideal characteristics of such filling materials. Namely, they may not provide an improved seal at the surface of the tooth structure and the cavity thereby preventing the migration of bacteria and material into the cavity or periapical tissues.
  • Some filling materials are not easily applied, are not able to form a structurally solid filling, are not sufficiently biocompatible, are not compatible with the presence of moisture, and/or are not easily sterilized.
  • MTA Mineral trioxide aggregate
  • gray or white ProRoot ® MTA (Dentsply International Inc., York, PA, US) is a substance that can be used in general dentistry and in endodontics to replace natural tooth material in apexification, pulp capping, pulpotomy, regenerative endodontics, root canal filling, root-end filling, root perforation repair, and apical barrier formation in teeth with necrotic pulps and open apices.
  • MTA has proven to be biocompatible and suitable for these procedures, MTA disadvantageously takes approximately three hours to set. This extended time for setting can require a patient to return for a second visit to complete treatment increasing the cost and inconvenience of treatment. Further, irrigating the operative field before the mineral trioxide aggregate has set can remove some of the mineral trioxide aggregate, thereby requiring an additional application of mineral trioxide aggregate.
  • the substance includes untreated MTA and anhydrous high-shear homogenized MTA ("homogenized MTA”) (prepared by a high- shear homogenization process involving high-shear and impact impingement of particles).
  • the substance includes untreated MTA, homogenized MTA, and water or a non-aqueous liquid, such as an alcohol.
  • MTA mineral trioxide aggregate
  • untreated mineral trioxide aggregate and “MTA” are used in accordance with their ordinary meaning in this field and include the substance generally sold under the trade name gray or white ProRoot ® MTA (Dentsply International Inc., York, PA, US).
  • MTA is mixture of a refined Portland cement and bismuth oxide, and may include a mixture of bismuth oxide, dicalcium silicate, tetracalcium aluminoferrite, tricalcium aluminate, and tricalcium silicate.
  • mineral trioxide aggregate includes the substance generally sold under the trade name white ProRoot ® MTA (Dentsply International Inc. , York, PA, US), which is similar in composition to gray ProRoot ® MTA except that white ProRoot ® MTA lacks tetracalcium alumino-ferrite.
  • a relatively short setting time can refer to a setting time of minutes rather than hours for a mineral trioxide aggregate.
  • a relatively short setting time can be between five minutes and twenty minutes, between ten minutes and twenty minutes, between ten minutes and fifteen minutes, between one and 10 minutes, or a clinically desirable setting time of minutes rather than hours for substances that replace natural tooth material.
  • the "maximum particle diameter” is used in accordance with its ordinary meaning in this field and includes largest diameter of the individual particle within an aggregate of particles.
  • median maximum particle diameter is used in accordance with its ordinary meaning in this field and includes a particle diameter at which about 50 wt. % of the sample has a smaller maximum particle diameter and about 50 wt. % of the sample has a larger maximum particle diameter.
  • the "dlO value" of a sample of aggregate is used in accordance with its ordinary meaning in this field and includes a diameter value that is greater than the maximum particle diameter of 10% of the particles in the sample.
  • the "d90 value" of a sample of aggregate is used in accordance with its ordinary meaning in this field and includes a diameter value that is greater than the maximum particle diameter of 90% of the particles in the sample.
  • homogenized is used in accordance with its ordinary meaning in this field and includes a sample produced through impingement of particles at high-shear rate and impact by high-shear homogenization.
  • a homogenized sample of aggregate can include particles produced by processes generally used in reducing particle size, such as, for example, air attrition milling, ball milling, jet milling, hydro milling, and attrition milling.
  • a homogenized sample of aggregate can include particles that are milled, ground, or granulated.
  • fineness is used in accordance with its ordinary meaning in this field and includes the granular size of cement particles.
  • untreated is used in its broad and ordinary sense and includes, for example, material not subject to particle size reduction processes such as high shear homogenization.
  • homogenized is used in its broad and ordinary sense and includes, for example, procedures that reduce particle size of materials, such as mineral trioxide aggregate, and/or narrow a distribution of particle sizes. "Homogenize” and “homogenized” do not mean that the material has a uniform particle size. Rather, homogenized material means that the material has been subjected to a homogenization process, such as high shear homogenization.
  • Characteristics of various embodiments of MTA mix e.g. radiopacity, sealing capacity, adaptability, adherence, biocompatibility, bioactivity, particle size, uniformity of the distribution, fineness, etc.
  • the various embodiments of MTA mixes including a combination of MTA compounds with different particle sizes and uniformities are described below with reference to FIGS. 2 and 5.
  • the MTA mix having a reduced set time can include varying ratios of MTA compounds with different particle sizes and uniformities and additives as described in detail in this application.
  • the leak-resistant MTA mix can include varying ratios of MTA compounds with different particle sizes and uniformities and additives as described in detail in this application.
  • the MTA mix can include an aqueous solution.
  • the example MTA mix embodiments disclosed herein can be suitable for use in other applications than those indicated when such applications involve similar dental, medical, veterinary or other environments involving moisture from bodily fluid.
  • the embodiments of MTA mix for orthograde filling are examples, and it is understood that other suitable MTA mixes can be used for the exemplary procedures described herein.
  • FIG. 1 depicts root canal therapy in a single-rooted tooth after apicoectomy and retrograde filling.
  • FIG. 1 depicts a cross-section of a healthy single-rooted tooth 10 with dentin 14 and enamel 16.
  • the retrograde cavity 18 is shown filled with a filling material.
  • the remainder of the pulp chamber 20 can be filled with standard obturating material such as gutta percha. In order to provide more sealing, the pulp chamber may also be sealed at the coronal end 22 with the filling material as shown in FIG. 1.
  • the remainder of the tooth cavity can be filled with a standard amalgam 24 or other permanent filling material.
  • retrofilling materials consist of many of the standard orthograde dental filling materials, and include gutta percha, zinc oxide eugenol paste, cavity, composite resins, gold foil, glass ionomers, standard amalgams, and other materials.
  • gutta percha zinc oxide eugenol paste
  • cavity composite resins
  • gold foil gold foil
  • glass ionomers standard amalgams
  • other materials The suitability of these materials as retrograde filling materials has been tested by their sealing ability, marginal adaption to the dentinal walls, biocompatibility, and clinical performance.
  • MTA Mineral trioxide aggregate
  • a bioactive material is one that elicits a specific biological response at the interface of the material resulting in the formation of a bond between the tissues and the material. If the material is nontoxic and biologically active, an interfacial bond may form between the material and living tissue.
  • Apatite-forming ability considered as an index of bioactivity (bond-to-bone ability), was tested on MTA after immersion in phosphate-containing solution (DPBS). MTA was able to form a superficial layer of apatite within hours, showing excellent bioactivity.
  • adding new chemicals can negatively affect the biocompatibility and bioactivity of MTA. Also, adding new chemicals can negatively affect the dimensional stability of MTA, such as its compressive strength and sealing capabilities. Another disadvantage of adding new chemicals can be the increase in time and cost in manufacturing and preparing of the dental substance. For example, use of high aluminate containing cement, sulfoaluminate cement, calcium fluoro-aluminate cement, or as reported 40-60% calcium aluminates in MTA which reduces setting times down to 15 minutes at the expense of calcium oxide, is a major disadvantage especially regarding the favorable effects of calcium hydroxide release on bacteria and caries. Under certain circumstances aluminum in high amounts is considered cytotoxic.
  • the present disclosure is directed to various types of fast- setting MTA compounds and mixes that do not compromise the clinical advantages normally associated with MTA.
  • the impact of particle size on setting time of MTA has not been previously described.
  • the suitability of a particular cement composition for a given purpose is typically determined by a combination of its chemical composition and its physical attributes, i.e. the manner and degree to which the cement is ground (granulation) and the resulting particle size.
  • the fineness of a cement is indicated by the cement's Blaine number, which represents the ratio of the cement's particle surface area to its weight (square centimeters of surface per gram).
  • Portland cements generally have a Blaine number in the range of 3,200 to 5,500 cm /g or greater.
  • the particle size of a cement is indicated by its median maximum particle diameter, which means that 50% of the sample has a smaller maximum particle diameter and 50% of the sample has a larger maximum particle diameter.
  • At least some embodiments of fast set MTA mix according to the present disclosure include untreated particles (hereinafter referred to as "untreated mineral trioxide aggregate” or “untreated MTA”) that were found to have a Blaine number in the range of 3,200-5,500 cm /g.
  • untreated mineral trioxide aggregate has a
  • untreated MTA was found to have a maximum particle diameter of greater than or equal to about 0.7 and/or less than or equal to about 42.2 microns with a median of 3.5 microns and a standard deviation of 4.1 microns.
  • the study was performed following ISO standard 6876:1986 for dental materials which specifies the requirements for dental materials used as filling materials.
  • the substance for use in general dentistry and in endodontics to replace natural tooth material.
  • the substance includes a combination of MTA compounds with different fineness.
  • the substance includes untreated MTA and homogenized MTA.
  • the homogenized MTA is anhydrous high-shear homogenized MTA, where the untreated MTA and anhydrous high-shear homogenized MTA together form an anhydrous fast set MTA mix.
  • FIG. 2 is a schematic diagram of a combination of MTA compounds each with a different fineness or particle diameters, in which untreated MTA 30 is mixed with homogenized MTA 32.
  • the relative particle sizes of the MTA particles shown in FIG. 2 are not drawn to scale, and it is understood that each of the particles can have any number of suitable particle size.
  • substances for a fast-setting filling material comprise a cement composition that can include bismuth oxide, dicalcium silicate, tricalcium aluminate, and tricalcium silicate.
  • the cement composition includes tertracalcium alumino-ferrite.
  • the cement composition includes calcium sulfate.
  • the cement composition includes Portland cement, or variations in the composition of such cement, which exhibit favorable physical attributes sufficient to form an effective seal against reentrance of infectious organisms.
  • the cement composition includes an aqueous liquid.
  • the aqueous solution comprises water.
  • the water comprises distilled water.
  • the water can include at least one of deionized water, filtered water, slurry water, and tap water.
  • the aqueous solution comprises a local anesthetic, such as lidocaine hydrochloride with or without epinephrine bitartrate. Other local anesthetic can also be used, as will be understood by a skilled artisan.
  • the substance, or cement composition is a leak- resistant MTA mix.
  • a leak-resistant MTA mix comprises bismuth oxide, dicalcium silicate, tricalcium aluminate, tricalcium silicate, and calcium sulfate.
  • combining the leak-resistant MTA mix with an aqueous solution produces a dental substance for use in general dentistry and in endodontics to replace natural tooth material.
  • the leak-resistant MTA mix comprises an anhydrous high-shear homogenized MTA comprising homogenized particles having a reduced median maximum particle diameter compared to an untreated MTA.
  • the leak- resistant MTA mix does not include additives that can compromise the biocompatibihty of the fast set MTA mix.
  • a medical grade anhydrous high-shear homogenized MTA is prepared by high-shear and impact impingement of particles using high-shear homogenization. In some embodiments, this process does not involve the use of grinding media.
  • the median maximum particle diameter of the untreated MTA is between about five and about thirty times larger than the median maximum particle diameter of the homogenized MTA.
  • the anhydrous high-shear homogenized MTA comprises bismuth oxide, dicalcium silicate, tricalcium aluminate, and tricalcium silicate.
  • a leak-resistant MTA mix comprises at least some calcium sulfate.
  • the quantity of calcium sulfate is greater than or equal to about 5 wt. % and/or less than or equal to about 15 wt. % of the leak-resistant MTA.
  • the leak-resistant MTA undergoes greater volumetric expansion during setting than MTA without the calcium sulfate.
  • the untreated MTA has a Blaine number that is greater than or equal to about 3,000 cm 2 /g, about 4,000 cm 2 /g, about 4,500 cm 2 /g, or even greater than or equal to about 5,000 cm /g. In some embodiments, the untreated MTA has a
  • Blaine number that is less than or equal to about 12,000 cm 2 /g, about 10,000 cm 2 /g, about
  • the untreated MTA has a Blaine number that is between about 3,000- 12,000 cm 2 /g, between about 4,000-11,000 cm 2 /g, between about 4,000-9,000 cm 2 /g, or even between about 5,000-5,500 cm 2 /g.
  • the anhydrous high-shear homogenized MTA has a
  • Blaine number that is greater than or equal to about 9,000 cm 2 /g, about 9,500 cm 2 /g, about
  • the homogenized MTA has a Blaine number that is less than or equal to about 300,000 cm /g or even less than or equal to about 20,000 cm /g.
  • the Blaine number of the untreated MTA compared to the Blaine number of the homogenized MTA is less than or equal to about three times or two times smaller. In some embodiments, the Blaine number of the untreated MTA is greater than or equal to about two times or five times the Blaine number of the homogenized MTA.
  • the untreated MTA has a median maximum particle diameter size of greater than or equal to about five times or even 8 times larger than the median maximum particle diameter size of the homogenized MTA. In some embodiments, the untreated MTA has a median maximum particle diameter size of less than or equal to about thirty times, 15 times, or even 12 times larger than the median maximum particle diameter size of the homogenized MTA.
  • the homogenized MTA has a dlO value that is greater than or equal to about 0.05 ⁇ , greater than or equal to about 0.055 ⁇ , greater than or equal to about 0.06 ⁇ , greater than or equal to about 0.08 ⁇ , greater than or equal to about 0.10 ⁇ , greater than or equal to about 0.12 ⁇ , greater than or equal to about 0.15 ⁇ , or even greater than or equal to about 0.19 ⁇ .
  • the homogenized MTA has a d90 value that is less than or equal to about 5.0 ⁇ , less than or equal to about 4.8 ⁇ , less than or equal to about 4.5 ⁇ , less than or equal to about 4.3 ⁇ , less than or equal to about 3.8 ⁇ , less than or equal to about 3.6 ⁇ , less than or equal to about 3.5 ⁇ , or even less than or equal to about 3.4 ⁇ .
  • the substance comprises greater than or equal to about 1 %, greater than or equal to about 10 wt. %, greater than or equal to about 15 wt. %, greater than or equal to about 20 wt. %, greater than or equal to about 25 wt. %, greater than or equal to about 40 wt. %, greater than or equal to about 45 wt. %, or even greater than or equal to about 55 wt. % untreated MTA.
  • the substance comprises less than or equal to about 99.9 wt. %, less than or equal to about 99.5 wt. %, less than or equal to about 99 wt. %, less than or equal to about 85 wt. %, or even less than or equal to about 75 wt. % untreated MTA.
  • the substance comprises greater than or equal to about 0.1 wt. %, greater than or equal to about 0.5 wt. %, greater than or equal to about 1 wt. %, greater than or equal to about 15 wt. %, or even greater than or equal to about 25 wt. % homogenized MTA. In some embodiments, the substance comprises less than equal to about 99 wt. %, less than or equal to about 90 wt. %, less than or equal to about 85 wt. %, less than or equal to about 80 wt. %, less than or equal to about 75 wt. %, less than or equal to about 60 wt. %, less than or equal to about 55 wt. %, less than or equal to about 45 wt. %, or even less than or equal to about 30 wt. % homogenized MTA.
  • the fast-setting MTA mix or substance comprises about 75 wt. % untreated MTA and about 25 wt. % homogenized MTA. In some embodiments, the substance comprises about 50 wt. % untreated MTA and about 50 wt. % homogenized MTA. [0093] In some embodiments, the substance comprising a solution of anhydrous fast set MTA mix comprises greater than or equal to about 50 wt. % or greater than or equal to about 80 wt. % anhydrous fast set MTA mix. In some embodiments, the solution comprises less than or equal to about 95 wt. % anhydrous fast set MTA mix. In some embodiments, the solution comprises greater than or equal to about 5 wt. % water and/or less than about 50 wt. % or even less than about 20 wt. % water
  • the substance comprises a leak-resistant MTA. In some embodiments, the substance comprises greater than or equal to about 5 wt. %, greater than or equal to about 6 wt. %, greater than or equal to about 8 wt. %, or even greater than or equal to about 10 wt. % calcium sulfate. In some embodiments, the substance comprises less than or equal to about 15 wt. %, less than or equal to about 12 wt. %, less than or equal to about 11 wt. %, or even less than or equal to about 10 wt. % calcium sulfate.
  • solutions according to the present disclosure comprises between about 50 wt. % about 95 wt. % anhydrous fast set MTA mix and between about 5 wt. % and about 50 wt. % water, where the anhydrous fast set MTA mix comprises between about 40 wt.% and about 99 wt. % untreated MTA and between about 1 wt. % and about 60 wt. % homogenized MTA.
  • the solution comprises between about 50 wt. % and about 95 wt. % anhydrous fast set MTA mix and between about 5 wt. % and about 50 wt. % water, where the anhydrous fast set MTA mix comprises between about 45 wt. % and about 75 wt. % untreated MTA and between about 25 wt. % and about 55 wt. % homogenized MTA.
  • a fast set solution comprises between about 50 wt. % and about 95 wt. % anhydrous fast set MTA mix and between about 5 wt. % and about 15 wt. % calcium sulfate, where the anhydrous fast set MTA mix comprises between about 40 wt. % and about 99 wt. % untreated MTA and between about 1 wt. % and about 60 wt. % homogenized MTA.
  • the solution comprises between about 50 wt. % and about 95 wt. % anhydrous fast set MTA mix and between about 5 wt. % and about 10 wt.
  • fast setting solutions comprise between about 50 wt. % and about 95 wt. % anhydrous fast set MTA mix and between about 5 wt. % and about 15 wt. % calcium sulfate, where the anhydrous fast set MTA comprises about 75 wt. % untreated MTA and about 25 wt. % homogenized MTA. In some embodiments, some solutions comprise between about 50 wt.
  • anhydrous fast set MTA mix comprises about 50 wt. % untreated MTA and about 50 wt. % homogenized MTA.
  • the substance for use in general dentistry and in endodontics to replace natural tooth material.
  • the substance can set within a tooth in a relatively short time, minutes rather than hours.
  • the substance includes a combination of anhydrous high-shear homogenized MTA and untreated MTA.
  • the substance can include an aqueous solution.
  • the setting time of the substance can be controlled by adjusting the fineness of the dental substance.
  • the fineness of the dental substance can be controlled by combining homogenized dental substance with untreated dental substance.
  • the fineness of the dental substance can be controlled by homogenizing the dental substance.
  • the fineness of the dental substance can be controlled by adjusting the number of homogenization cycles to which the dental substance is subjected.
  • the setting time of the substance can be controlled by adjusting the uniformity of the particle sizes of the dental substance.
  • the uniformity of the particle sizes of the dental substance can be controlled by combining homogenized dental substance with untreated dental substance.
  • the uniformity of the dental substance can be controlled by homogenizing the dental substance.
  • the uniformity of the dental substance can be controlled by increasing or decreasing homogenization cycles when homogenizing at least a portion of the dental substance.
  • Some embodiments provide a method of making a substance for use in general dentistry and in endodontics to replace natural tooth material, where the substance expands during setting.
  • the method includes mixing MTA with calcium sulfate, which can reduce leakage.
  • the methods include adding calcium sulfate to an anhydrous fast set MTA mix that includes untreated MTA and homogenized MTA.
  • an anhydrous fast set MTA mix when mixed with an aqueous solution, experiences moderate expansion (about 0.5% volumetric expansion) during setting without the calcium sulfate.
  • the anhydrous fast set MTA mix can be expanded during setting by adding an expansion agent.
  • the expansion agent is calcium sulfate. In some embodiments, expansion and setting may happen simultaneously.
  • the amount of expansion can be controlled by increasing or decreasing the amount of calcium sulfate. When calcium sulfate is added in certain concentrations, the amount of expansion can be increased. Controlling the amount of calcium sulfate can control the degree of expansion, and can thus reduce leakage by having the dental filling expand to a desired degree. In some embodiments, the dental substance, by adding calcium sulfate, can undergo volumetric expansion of greater than about 0.5% during setting.
  • Methods of reducing the particle size of a dental substance including reduction of particle size by using high shear homogenization are described below with references to FIGS. 3 and 4.
  • the methods of reducing particle size of dental substance using high shear homogenization can include any of the steps as described in detail in this application. Any of the steps described below can be incorporated into any of the methods described in FIG. 3.
  • the method of reducing particle size can include creating a suspension of the dental substance and a non-aqueous liquid.
  • the steps disclosed herein can be suitable for use in other applications than those indicated when such applications involve shortened particle size reduction time and reduction of particle size to a similar degree of uniformity.
  • Some embodiments disclosed herein provide a method of making a substance for use in general dentistry and in endodontics to replace natural tooth material, where the substance sets in a relatively short time.
  • methods of making such a substance include reducing the particle size of the substance.
  • the methods include homogenizing by high-shear and impact impingement of particles to reduce particle size, thereby producing anhydrous high-shear homogenized MTA.
  • FIG. 3 illustrates a method 300 for homogenizing particle sizes of an MTA material.
  • an MTA material which may include a previously untreated MTA material, is mixed with a non-aqueous liquid or solution to achieve a suspension of the MTA material.
  • the suspension may be actively mixed or agitated to avoid or reduce concentration gradients within the suspension.
  • the suspension is placed into a reservoir of a machine configured to homogenize particles, such as through by high-shear and impact impingement of particles.
  • a pump is then operated at step 330 to apply a force to the suspension.
  • the suspension at step 340 is forced through one or more channels or microchannels thereby causing at least some of the MTA particles to contact the channel walls and/or each other.
  • the friction and impact of such contact causes at least some particles to break apart or to be reduced in size.
  • a reduction in size results in an increase in the particle's Blaine number.
  • the solution is circulated through the machine as many times as desired to achieve a particular size and/or size distribution of the MTA particles. Once the desired size or size distribution has been achieved, the non-aqueous portion of the suspension is allowed to evaporate at step 360 leaving behind an anhydrous high- shear homogenized MTA product.
  • the non-aqueous solution or liquid used in step 310 is an alcohol.
  • the alcohol includes at least one of methanol, ethanol, and isopropanol.
  • the liquid is ethanol.
  • operating a pump at step 330 accelerates the suspension into an interaction chamber under high pressure.
  • methods include circulating the suspension at step 350 forced through the channel into the inlet reservoir between two and two hundred times, two and one hundred times, between two and fifty times, or even between 5 and thirty times.
  • method 300 can be performed without the use of grinding media, such as a ball mill.
  • the MTA material can be mixed at step 310 with the liquid in a ratio of between about 1 part material to between about 1 and 100 parts liquid. In some embodiments, the material can be mixed with the liquid in a ratio of between about 1 part material to between about 1 and 20 parts liquid. In some embodiments, the material can be mixed with the liquid in a ratio of between about 1 part material to between 5 and 20 parts liquid. In some embodiments, the material can be mixed with the liquid in a ratio of between about 1 part material to between 5 and 10 parts liquid. In some embodiments, the material can be mixed with the liquid in a ratio of 1 part material to 9 parts liquid.
  • mixing the material with a liquid includes using a magnetic stir bar to produce a suspension.
  • placing the mixture of material and liquid into the machine includes pouring the mixture into a reservoir of the machine.
  • the reservoir can include a device for preventing premature settling of the mixture which could cause a concentration gradient within the machine or a part of the machine, and the method can include actuating the device.
  • the device can be an overhead propeller.
  • homogenizing the material within the mixture includes using a pressure greater than or equal to about 1000 psi and/or less than or equal to about 70,000 psi. In some embodiments, homogenizing the material within the mixture includes forcing particles through the channel using pressure greater than or equal to about 25,000 psi and/or less than or equal to about 40,000 psi. In some embodiments, homogenizing the material within the mixture includes using a pressure of about 30,000 psi.
  • the method includes evaporating the liquid from the homogenized material.
  • the liquid is ethanol
  • evaporating the liquid from the homogenized material includes placing the homogenized material and liquid in an oven at 65 °C for a sufficient time to evaporate at least some of the ethanol or to substantially remove the ethanol.
  • evaporating the liquid from the homogenized material includes letting the samples sit at room temperature in a fume hood with a vacuum pulled over the bottles.
  • the method includes collecting the homogenized material after subjecting it to a homogenizing process.
  • a method of making a substance for use in general dentistry and in endodontics to replace natural tooth material includes homogenizing particles by high- shear and impact impingement to reduce particle size.
  • methods include, first, selecting a material suitable for use in the method to make a substance for use in general dentistry and in endodontics to replace natural tooth material, where the material includes particles having a Blaine number, and/or a median maximum particle diameter.
  • the material is an MTA material, such as for example gray ProRoot® MTA available from Dentsply International Inc., York, PA, US.
  • the method includes mixing the selected material with a liquid creating a mixture of the material and liquid.
  • a liquid can be used in homogenizing by high-shear and impact impingement: however, water is not used in some embodiments as it may cause the material to set prematurely. Therefore, in some embodiments, the liquid is non-aqueous. In some embodiments, the liquid is an alcohol, though any suitable non-aqueous liquid can be used as will be understood by those with skill in the art.
  • the method includes providing a machine for homogenizing by high-shear and impact impingement of particles.
  • the machine provided is an M-110EH Microfluidizer® (Microfluidics, Newton, MA, US), though any suitable machine for homogenizing by high-shear and impact impingement of particles may be used, as will be understood by those with skill in the art.
  • the reservoir of the homogenization machine includes a device for preventing premature settling of the mixture which could cause a concentration gradient within the machine or a part of the machine, and the method includes actuating the device to prevent premature settling of the mixture which would cause a concentration gradient within the machine or a part of the machine.
  • the device is an overhead propeller.
  • the method comprises homogenizing by high-shear and impact impingement of particles rather than by using ball milling as is currently used.
  • Ball milling involves contacting the particles to be reduced in size with grinding media in a chamber, where the grinding media is different in composition from the particles, and where repeated contact with the grinding media reduces the size of the particles, thereby producing homogenized particles.
  • the grinding media is frequently one or more than one ball, such as for example one or more than one glass ball, from which the method is named.
  • homogenizing by high-shear and impact impingement of particles involves forcing particles through a channel using pressure, where repeated contact of the particles to be reduced in size with each other and with the pressure and the channel walls reduces the size of the particles, thereby producing homogenized particles.
  • the method of homogenizing by high-shear and impact impingement of particles produces homogenized particles that have unexpected advantages over other used methods, in particular decreasing the setting time of the homogenized particles, as disclosed in this disclosure, when the homogenized particles are used by themselves or when the homogenized particles are combined with untreated particles in general dentistry and in endodontics to replace natural tooth material.
  • homogenizing by high-shear and impact impingement of particles requires less time to reduce particle sizes than does ball milling. Further, pieces of the grinding media used in ball milling can contaminate the homogenizing particles produced as the grinding media wears, while the method of homogenizing by high-shear and impact impingement of particles does not use grinding media that can contaminate the homogenized particles produced.
  • particles of dental material should be substantially free of contaminants after being processed.
  • the particle size reduction of the milled particles produced by ball milling can be less uniform than the particle size reduction of the homogenized particles produced by homogenizing by high-shear and impact impingement of particles, and the decreased uniformity of the milled particles produced by ball milling increases their setting time as compared with the setting time for homogenized particles produced by homogenizing by high-shear and impact impingement of particles using high-shear homogenization that have a more uniform size.
  • the particle sizes of the milled particles produced by ball milling are generally larger than the particle sizes of the homogenized particles produced by homogenizing by high-shear and impact impingement of particles. High-shear homogenization produces fewer large particles, i.e.
  • the larger particle size of the milled particles produced by ball milling increases their setting time as compared with the setting time for homogenized particles that have a smaller particle size produced by homogenizing by high-shear and impact impingement of particles.
  • machines used in ball milling can be more difficult to clean in preparation for reuse than machines used in homogenizing by high-shear and impact impingement of particles, because in ball milling the milled particles may need to be separated from the grinding media, where in homogenizing by high-shear and impact impingement of particles, the milled particles can be merely flushed out of the machine as there is no grinding media. Because of these advantages, homogenizing by high-shear and impact impingement of particles can be more efficient and cost effective than ball milling for making a substance for use in general dentistry and in endodontics to replace natural tooth material.
  • the untreated MTA had a median maximum particle diameter size approximately five to eight times the median maximum particle diameter size of the milled MTA.
  • the study was performed following ISO standard 6876: 1986 for dental materials which specifies the requirements for dental materials used as filling materials.
  • the anhydrous high-shear homogenized mineral trioxide aggregate was prepared as follows. Untreated MTA (gray ProRoot MTA) was obtained from Dentsply International Inc. (York, PA, US). The starting median particle size for the untreated MTA was determined to be 3.8 microns. The untreated MTA was mixed with ethanol in a ratio of 1 to 9 by weight using a magnetic stir bar to produce a suspension. The suspension was poured into the inlet reservoir of a machine that homogenizes by high-shear and impact impingement of particles, such as, for example, an M-110EH Microfluidizer ® (Microfluidics, Westwood, MA, US) with an overhead propeller mixer also in the reservoir.
  • M-110EH Microfluidizer ® Microfluidics, Westwood, MA, US
  • the overhead propeller mixer was used to prevent premature settling that could cause a concentration gradient in the check-valve of the processor due to the high density of MTA.
  • the suspension was forced at extreme high shear through a very small diamond orifice.
  • the high shear up to 40,000 psi delivers the product into the interaction chamber using a constant pressure pumping system.
  • Precisely engineered microchannels within the chamber range from 50-500 microns and generate shear and impact forces that cause homogenization and de- agglomerates the MTA particles.
  • the temperature was regulated by a heat exchanger, and the lack of moving parts maximizes uptime.
  • the untreated MTA used in the experiment was measured twice.
  • the untreated MTA sample was found to have a d90 value (i.e. 90% of the material is this size or smaller) of 10.73 ⁇ , and 22.157 ⁇ .
  • the untreated MTA sample was found to have a dlO value (i.e. 10% of the material is this size or smaller) of 0.867 ⁇ , and 1.045 ⁇ .
  • the median maximum particle diameter size of the untreated MTA was reduced to 0.49 microns after fifty passes, thereby producing the anhydrous high-shear homogenized MTA, or approximately an eight-fold reduction in median particle size.
  • the particle size of the MTA was reduced to have a d90 value of 3.292 ⁇ and a dlO value of 0.359 ⁇ . After ten passes, the particle size of the MTA was reduced to have a d90 value of 1.461 ⁇ and a dlO value of 0.281 ⁇ . After twenty passes, the particle size of the MTA was reduced to have a d90 value of 1.147 ⁇ and a dlO value of 0.22 ⁇ . After thirty passes, the particle size of the MTA was reduced to have a d90 value of 0.95 ⁇ and a dlO value of 1.191 ⁇ .
  • the particle size of the MTA was reduced to have a d90 value of 1.18 ⁇ and a dlO value of 0.195 ⁇ . After fifty passes, the particle size of the MTA was reduced to have a d90 value of 1.301 ⁇ and a dlO value of 0.195 ⁇ . Table 1 lists the processing conditions and particle size measurements.
  • FIG. 4 is a schematic graph showing particle size distributions of untreated MTA 410 compared with samples of homogenized MTA.
  • a sample of homogenized MTA 420 produced by cycling the untreated MTA ten times reduces the median maximum particle size of the MTA to below 1 ⁇ . Passing the untreated MTA 20 times (line 430), 30 times (line 440), and 50 times (line 450) produced samples having finer particles.
  • the ethanol used to form the solution was then evaporated off in an oven at 65 °C and the solids were collected for analysis of the effects of adding the homogenized MTA to untreated MTA on the setting time of untreated MTA.
  • the ethanol can be evaporated off by letting the samples sit at room temperature in a fume hood with a vacuum pulled over the bottles. In such case, the samples may not need to be at elevated temperatures, as long as a vacuum is used and the samples are being left to dry for a sufficient amount of time. Table 2 shows the results of this study. TABLE 2
  • the minimum amount is used of homogenized MTA in the substance suitable for reducing setting time to a clinically acceptable amount, as will be understood by those with skill in the art.
  • FIG. 5 is a schematic graph showing generally linear relationship 510 between setting time and particle size.
  • FIG. 5 also illustrates at least one clinically desired range 520 of setting times of dental substances. Because of the relationship 510 between particle size and set time, selecting a set time within range 520 dictates that particles sizes within range 530 may be achieved through a homogenization process.
  • the dental procedures using MTA may have a clinically desired setting time of more than six minutes, in some cases between ten and fifteen minutes. Thus, in some embodiments, the minimum amount of homogenized MTA may be determined as disclosed herein to achieve a desired setting time.
  • distilled water is non-toxic in the clinical setting, inexpensive, and readily available, distilled water can be used as the MTA combination solvent to prepare a dental substance from a fast set MTA mix disclosed herein.
  • Methods of using a fast-setting dental substance are described below with reference to FIG. 6.
  • the methods of using a fast-setting dental substance can include any of the steps as described in detail in this application. Any of the steps described below can be incorporated into any of the methods described in FIG. 6.
  • the method of using a fast-setting dental substance can include allowing the dental substance to set within five to twenty minutes.
  • the steps disclosed herein can be suitable for use in other applications than those indicated when such applications involve using a dental substance that sets within a short time.
  • methods include performing a dental procedure.
  • the dental procedure is an endodontic procedure.
  • the dental procedure includes removing part of the natural tooth material of a tooth.
  • the dental procedure can include removing material that replaced natural tooth material.
  • the dental procedure includes at least one of the following: apexification, pulp capping, pulpotomy, regenerative endodontics, root canal filling, root-end filling, root perforation repair, and apical barrier formation in teeth with necrotic pulps and open apices.
  • FIG. 6 is a flow chart outlining a method for using a dental substance according to some embodiments of the present disclosure.
  • method 600 includes performing a dental procedure at step 610, providing a dental substance comprising fast set mineral trioxide aggregate mix and using the substance to fill a space in the tooth at step 620, and allowing the substance to set at step 630.
  • the dental procedure can further include, after allowing the dental substance to set, adjusting the height of the dental substance in the tooth (not shown).
  • the dental procedure can further include, after allowing the dental substance to set, carving the dental substance (not shown).
  • the dental procedure includes delivering the dental substance to the canal orifice, pushing the dental substance into the canal orifice, pushing a spreader into the root canal, filling the root canal with the dental substance, and sealing the root canal using the dental substance.
  • the dental procedure includes utilizing a temporary filler for the remainder of the cavity, and replacing the temporary filler with the desired permanent filling material.
  • the dental procedure includes introducing the sealing material into the root end cavity whereby the path of communication between the root canal and outer surface of the tooth is sealed.
  • the dental procedure includes filling the root perforation with the filling material whereby said filling material seals the path of communication between the other surface of the tooth and the canal of the tooth.
  • the methods include providing a substance comprising fast set MTA mix. In some embodiments, the methods include using the substance to fill a space in the tooth, and allowing the substance to set. In some embodiments, the methods include, before using the substance to fill a space in the tooth, filling the tooth with an additive.
  • the additive comprises a radiopaque material, such as a phosphate. Other radiopaque materials can also be used, as will be understood by those with skill in the art.
  • the methods include orthograde filling.
  • the methods include, after allowing the dental substance to set, adjusting the height of the dental substance in the tooth.
  • the method include, after allowing the dental substance to set, carving the dental substance.
  • the dental procedure is an endodontic procedure.
  • the dental procedure is a retrograde canal filling.
  • the dental procedure is an orthograde canal filling.
  • the dental procedure includes removing part of the natural tooth material of a tooth.
  • the dental procedure includes removing material that replaced natural tooth material.
  • the dental procedure includes at least one of an apicoectomy, a root perforation sealing, an apexification, a pulp capping, a pulpotomy, regenerative endodontics, a root canal filling, a root-end filling, a root perforation repair, and an apical barrier formation in teeth with necrotic pulps and open apices.

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  • Veterinary Medicine (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Plastic & Reconstructive Surgery (AREA)
  • Dental Preparations (AREA)

Abstract

L'invention concerne, dans des modes de réalisation, une substance qui durcit en un délai relativement court et destinée à être utilisée en dentisterie générale et en endodontie pour remplacer un matériau de dent naturelle. La substance peut comprendre un mélange d'agrégat de trioxyde minéral non traité et d'agrégat de trioxyde minéral anhydre homogénéisé par cisaillement élevé. Dans certains modes de réalisation, la substance comprend un agrégat de trioxyde minéral non traité, un agrégat de trioxyde minéral anhydre homogénéisé par cisaillement élevé, et de l'eau. Une méthode de fabrication d'une substance qui durcit en un délai relativement court et destinée à être utilisée en dentisterie générale et en endodontie pour remplacer un matériau de dent naturelle peut consister à homogénéiser des particules par cisaillement élevé et par des chocs. Les modes de réalisation de la présente invention comprennent des méthodes permettant d'utiliser un mélange d'agrégat de trioxyde minéral homogénéisé à durcissement rapide en dentisterie générale et en endodontie pour remplacer un matériau de dent naturelle.
PCT/US2015/014271 2014-02-05 2015-02-03 Substances et méthodes de remplacement d'un matériau de dent naturelle Ceased WO2015119954A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US201461936223P 2014-02-05 2014-02-05
US61/936,223 2014-02-05
US201461974350P 2014-04-02 2014-04-02
US61/974,350 2014-04-02

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021009369A1 (fr) * 2019-07-18 2021-01-21 Septodont Ou Septodont Sas Ou Specialites Septodont Ciment hydraulique dentaire comprenant des particules ultrafines de silicate de calcium présentant un durcissement rapide et des propriétés mécaniques appropriées
WO2023205886A1 (fr) * 2022-04-26 2023-11-02 Pds Inc. Matériau d'obturation d'agrégat de trioxyde minéral amélioré pour dentisterie et dispositif pour son utilisation
RU2831730C2 (ru) * 2019-07-18 2024-12-12 Септодон У Септодон Сас У Спесилите Септодон Набор для получения дентального восстанавливающего материала, дентальная композиция, медицинское устройство

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US5769638A (en) * 1993-04-23 1998-06-23 Loma Linda University Tooth filling material and method of use
DE10021605A1 (de) * 2000-05-04 2001-11-08 Upmeyer Hans Juergen Füllmaterial für Zähne
US20050263036A1 (en) 2001-01-04 2005-12-01 Primus Carolyn M Dental material
WO2013142608A1 (fr) * 2012-03-21 2013-09-26 Loma Linda University Substances et procédé destinés à remplacer du matériau dentaire naturel

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5769638A (en) * 1993-04-23 1998-06-23 Loma Linda University Tooth filling material and method of use
DE10021605A1 (de) * 2000-05-04 2001-11-08 Upmeyer Hans Juergen Füllmaterial für Zähne
US20050263036A1 (en) 2001-01-04 2005-12-01 Primus Carolyn M Dental material
WO2013142608A1 (fr) * 2012-03-21 2013-09-26 Loma Linda University Substances et procédé destinés à remplacer du matériau dentaire naturel

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021009369A1 (fr) * 2019-07-18 2021-01-21 Septodont Ou Septodont Sas Ou Specialites Septodont Ciment hydraulique dentaire comprenant des particules ultrafines de silicate de calcium présentant un durcissement rapide et des propriétés mécaniques appropriées
CN114514210A (zh) * 2019-07-18 2022-05-17 塞普托东专业股份有限公司 包含具有快速硬化和合适机械性能的超细硅酸钙颗粒的牙科水硬性黏固剂
JP2022541269A (ja) * 2019-07-18 2022-09-22 セプトドント ウ セプトドント サ ウ スペシャリテ セプトドント 急速硬化し、かつ好適な機械的特性を有する超微粒ケイ酸カルシウム粒子を含む歯科用水硬性セメント
RU2831730C2 (ru) * 2019-07-18 2024-12-12 Септодон У Септодон Сас У Спесилите Септодон Набор для получения дентального восстанавливающего материала, дентальная композиция, медицинское устройство
JP7684273B2 (ja) 2019-07-18 2025-05-27 セプトドント ウ セプトドント サ ウ スペシャリテ セプトドント 急速硬化し、かつ好適な機械的特性を有する超微粒ケイ酸カルシウム粒子を含む歯科用水硬性セメント
WO2023205886A1 (fr) * 2022-04-26 2023-11-02 Pds Inc. Matériau d'obturation d'agrégat de trioxyde minéral amélioré pour dentisterie et dispositif pour son utilisation

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